Meta phenylenediamine 4 sulphonic acid (MPDSA) is one of the important products in the dyestuff sector. The present conventional manufacturing process for MPDSA being carried out at the industry is less efficient and gives an overall yield of about 60 %. But the use of alternative raw materials for the manufacture of MPDSA can give yield as high as upto 80%. In addition, this process also eliminates the use of metal catalysts which cause downstream problems. This method involves the use Metaphenylene Diamine as the raw material instead of 2, 4, dinitrochlorobenzene for the manufacture of MPDSA. A lab scale experiment has been carried out and the overall yield has been found to be higher than that obtained from the conventional process. This paper describes this new manufacturing process and its possible economic benefits. Overall yield is calculated and compared with the conventional process.

1. IJSRD - International Journal for Scientific Research & Development| Vol. 1, Issue 2, 2013 | ISSN (online): 2321-0613
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Increasing Yield in the Manufacturing of MPDSA
Mehul T. Chauhan 1
Prof. R. N. Shukla2
Prof. Hiral N. Pandya3
1,2,3
L. D. College of Engineering, Ahmedabad, Gujarat, India
Abstract— Meta phenylenediamine 4 sulphonic acid
(MPDSA) is one of the important products in the dyestuff
sector. The present conventional manufacturing process for
MPDSA being carried out at the industry is less efficient
and gives an overall yield of about 60 %. But the use of
alternative raw materials for the manufacture of MPDSA
can give yield as high as upto 80%. In addition, this process
also eliminates the use of metal catalysts which cause
downstream problems. This method involves the use
Metaphenylene Diamine as the raw material instead of 2, 4,
dinitrochlorobenzene for the manufacture of MPDSA.
A lab scale experiment has been carried out and the overall
yield has been found to be higher than that obtained from
the conventional process. This paper describes this new
manufacturing process and its possible economic benefits.
Overall yield is calculated and compared with the
conventional process.
Key words – Meta phenylene diamine 4 Sulphonic acid,
Oleum 23%, Oleum65%
I. INTRODUCTION
Dye Intermediates: The precursors of dyes are called dye
intermediates. They are obtained from simple raw materials,
such as benzene and naphthalene, by a variety of chemical
reactions.
Usually, the raw materials are cyclic aromatic
compounds, but acyclic precursors are used to synthesize
heterocyclic intermediate acid which is a by-product of the
process. Are derived from two principal sources, coal tar
and petroleum. [1]
The first synthetic dye, Mauveine, was discovered
by Perkin in 1856. Hence the dyestuffs industry can rightly
be described as mature. However, it remains a vibrant,
challenging industry requiring a continuous stream of new
products because of the quickly changing world in which we
live. The early dyes industry saw the discovery of the
principal dye chromo gens (the basic arrangement of atoms
responsible for the color of a dye). Indeed apart from one or
two notable exceptions, all the dye types used today were
discovered in the nineteenth century. The introduction of the
synthetic fibers, nylon, polyester, and polyacrylonitrile
during the period 1930-1950. [2]
sativa L). Section 3 talks
about the materials and methods proposed for calculating
parameters for the quality of rice seeds (Oryza sativa L).The
proposed system and proposed algorithm for computing
Rice seed (Oryza sativa L)with long seed as well as small
seed being present in the sample is also discussed in the
same section. Section 4 discusses the quantification for the
quality of rice seeds based on image processing and
analysis. Section 5 discusses results based on quality
analysis. Section 6 provides the conclusion of the proposed
process.
II. MANUFACTURING PROCESS IN PLANT
Process Step:-A.
1) Sulphonation Process:
1000 kg 2, 4 DNCB is partially sulfonated with 625 kg
sodium bisulphite in presence of 150 kg magnesium oxide in
reaction vessel under constant stirring condition.
PH is maintained at 7 to7.5 and temperature maintained at
52o
C for 8 hour.
After Cooling, adding 1700 kg salt, filter,
centrifugal, get 1200 kg 2, 4 dinitrobenzene sulphonic acid
(Nitro mass).
2) Reduction of nitro mass:
 1200 Kg 2, 4-dinitrobenzenesulfonic acid is taken into
the reduction vessel which contains 1100 kg scrap
iron and hydrochloric acid. After boiling, maintain
temperature at 99o
C
 After reaction completion, mass is sent to a filter press
 Finally, Centrifugal and drying gives 600 kg MPDSA.
III. YIELD IMPROVEMENT METHOD FROM
LITERATURE.
(1) Use of Agitated Nutche Filter by Equipment changing.
(2) Use of spray dryer with scrubber
(3) Using Different catalyst instead of Fe (iron powder) in
reduction process. Like Zno (Zinc oxide), platinum,
palladium, Raney nickel, polysulfide (caustic+sulfer) etc.
can be used. [11]

2. Increasing yield in the manufacturing of MPDSA
(IJSRD/Vol. 1/Issue 2/2013/0020)
All rights reserved by www.ijsrd.com 131
(4) Recycle of mother liquor for reduction process
(5) Raw material changes process modification
IV. IMPROVING YIELD BY PROCESS
MODIFICATION
Principal:-Solid m phenylene diamine (MPD), about 98-99
%.is sulfonated with 20% Oleum to m-phenylene Diamine
4-sulfonic acid and partly to some 4:5 and 4:6 isomer which
are subsequently hydrolyzed by boiling with weekend
sulfuric acid to monosulfonic acid, thus resulting in the
formation of the objective compound.[13]
The hydrolysis batch is finally drowned into an ice water
mixture and the precipitated product is filtered thought
nutch filter the wet product is further sucked in hydro
extractor to raise the solid contents. The centrifuged cakes
are finally evaluated for real content and the yield
calculated.
The product is used or solid in form of wet cake. [4]
V. FIGURE: EXPERIMENTAL SETUP
Apparatus:
Thermometer, Borosilicate glass 1000ml sspl 3 neck flask,
(round bottom flask.),Separation funnel, Magnetic stirrer,
Beaker, Flask, funnel, Heater mantle.
Raw material:
1 Mpd= 70 gm
2. 98% H2SO4 =118 ml
3. 25% Oleum=40 ml
4. 60% Oleum=100 ml
5. Common solt =16 gm
STEP:-
1) Take a 1000 ml capacity of 3 neck flask (Round bottom
flask) having stirrer with connected with electric motor.
2) Adding 118ml of 98% sulfuric acid and 40 ml of 25%
Oleum in round bottom flask. In under Stirring condition.
3) After 23% Oleum addition, gradually add 70 gm real
Dry m phenylene diamine
(M..Wt. 108.0) over a period of about 1 hour, maintain the
temperature between 85°C -90 °C.
4) Then add to 100 of 60% Oleum over a period of 1 ½
hour.
Heat the Sulphonation mass to 156°C during about 4
hours. And maintain it for 3 hour. Now Sulphonation is
positively complete.
5) Now cool the mass to 88°C by adding ice externally.
Hydrolysis of disulfonic acid isomer
6) Now charge 18 ml water drop by drop to the
sulfonation mass for 1 hour.
7) Maintaining the temp between 85°C to 90°C
8) Now heat the mass gradually 135°C for 4 hour, and
then cool the mass to 85 °C
9) Take a separate beaker and add 120 ml water and 480
gm of ice.
10) Then transfer the content from the sulfonater to beaker
at that time temperature is 40°C to 50 °C
11) Cool the batch 30 °C to 2hour gradually and further
18°C in a 4 hour.
Filtration:-
12) Filter the batch and wash the cakes by 60 ml of as is
25% weight/vol brine. Centrifuge the wet cakes to further
suck down the liquor. Weight the centrifuge wet cakes and
record.
13) Check sample of centrifuge wet cake and determine its
real content calculation and record yield.
VI. RESULTS
Weight the centrifuge wet cakes :- ( Total cake mass)
= 185 gm
Moisture =40% = 77.6 gm
Dry mass = 107.4gm
UN reacted MPD=8% = 14.8 gm
MPDSA REAL = 92.6 gm.
• Calculation of yield :-
 Initially weight taken of m-phenylene diamine
70 gm

3. Increasing yield in the manufacturing of MPDSA
(IJSRD/Vol. 1/Issue 2/2013/0020)
All rights reserved by www.ijsrd.com 132
 According to that moles of m-phenylene diamine
0.6481 mole
 After that, for step-2 disulfonic acid isomer is send
for hydrolysis, and at final end product produce is
Meta phenylene diamine sulfonic acid.
 Total weight of MPDSA product is 92.6gm
 Molecular weight of MPDSA is 188gm/mol
 So, total mole of MPDSA product is 0.4925 moles.
Moles of MPD reacted to produce
(moles of MPDSA)
MPDSA %Yield = -------------------------------------------------
. Total moles of MPD initially
0.4925
= ----------------- * 100
0.6481
ANS= 75.99% yield
Comparison of exp results with plant data
1) Yield of MPDSA:
Process Yield
Plant 60%
Experiment 76%
VII. CONCLUSION
In company, we get yield of MPDSA as 60%. In this
experiment, Meta phenylene diamine was used instead of 2,
4 dinitrochlorobenzene as raw material and the yield was
found to be about 75%. The yield can be further increased to
85% by allowing Sulphonation to occur for 2 more hours.
REFERENCES
[1]
Kirk Othmer, ‘encyclopedia of chemical technology’
(1965), Volume8 4th edition. Page no: 299,300,301
[2]
Company: Rakesh Chemical Industries Naroda GIDC.
[3]
B.G.NAIK,‘Plant process of pharmaceutical and dyestuff
inter mediate ’ Chap: 17, page no: 97, 98
[4]
K.R.DESAI ,‘Plant process .of pharmaceutical and
dyestuff intermediate ’ Chep: 17, page no: 97, 98
[5]
K.A.GAVANE ‘introduction to process calculation
stoichiometry’